616-23-9Relevant academic research and scientific papers
Effect of sodium chloride on the solubility and hydrolysis of epichlorohydrin in water
Dmitriev,Zanaveskin,Khadzhiev
, p. 1627 - 1630 (2018)
The mutual solubility of the components in the epichlorhydrin–water–sodium chloride system was studied in the temperature range of 20–90 °С. It was found that epichlorohydrin is salted out as the concentration of NaCl increases. The Sechenov coefficient was determined to be equal to 0.29. It was found that epichlorohydrin reacts with an aqueous solution of sodium chloride to form glycerol dichlorohydrins. Alkali formed during this reaction catalyzes the hydrolysis of epichlorohydrin to glycerol monochlorohydrin, acts as a reagent in the glycidol formation and accelerates its subsequent conversion to glycerol.
Preparation method for 1,3-propylene glycol from glycerol
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Paragraph 0066-0076, (2021/04/10)
The invention relates to a preparation method for 1,3-propylene glycol from glycerol, wherein the preparation method comprises the steps of chlorohydrination reaction, cyclization reaction, hydrogenation reaction and the like. The glycerin conversion rate of the preparation method reaches 99% or above, the yield of 1,3-propylene glycol reaches 65% or above, and the preparation method has the advantages of being simple in process, mild in reaction condition, small in investment, high in technical safety and easy to operate and control.
A safer and greener chlorohydrination of allyl chloride with H2O2 and HCl over hollow titanium silicate zeolite
Peng, Xinxin,Xia, Changjiu,Lin, Min,Shu, Xingtian,Zhu, Bin,Wang, Baorong,Zhang, Yao,Luo, Yibin,Mu, Xuhong
, p. 17 - 25 (2017/06/23)
Industrial production of dichloropropanols through chlorohydrination of allyl chloride suffers from a series of disadvantages such as use of hazardous Cl2, low atom economy, low dichloropropanol concentration and serious pollution. In this work, a safer and greener route for chlorohydrination of allyl chloride with H2O2 and HCl over hollow titanium silicate (HTS) at mild condition is developed. Unlike the traditional Cl2-based chlorohydrination, this novel method is initiated via synergistic effect of Lewis acidity (HTS) and Br?nsted acidity (HCl) to promote occurrence of oxidation, protonation and nucleophilic reaction of allyl chloride simultaneously and hence dichloropropanols are generated. Owing to a completely different reaction route, the formation of 1,2,3-trichloropropane by-product is depressed and the content of dichloropropanol exceeded 22?wt%, which increase by about 4 times compared with traditional Cl2-based chlorohydrination (the content of dichloropropanol is below 4?wt%). At the optimized conditions, both of the allyl chloride conversion and dichloropropanol selectivity could approach 99% simultaneously and the waste is minimized. What's more, the HTS was reusable. Concentrated HCl solution treatment was adopted to test HTS's stability. The characterization and catalytic evaluation results reveal that, although parts of the framework Ti species have transformed into non-framework Ti and then leached into the solution, HTS remains structural stable, and the allyl chloride conversion and dichloropropanol selectivity didn't decrease obviously during the treatment.
Method for comprehensive utilization of hexachloroethane
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Paragraph 0015; 0017-0019; 0021; 0023; 0025; 0027; 0030, (2017/10/27)
The invention relates to a comprehensive utilization method of a dichloroethane chlorination byproduct namely hexachloroethane. The comprehensive utilization method comprises the following steps: adding a hexachloroethane solution, glycerin, a hydrogenation catalyst and a chlorination catalyst into a high-pressure kettle; after feeding is finished, performing hydrodechlorination and glycerin chlorination reaction at the same time at certain temperature and under certain hydrogen pressure; after reaction is finished, maintaining the temperature for 4h, and then reducing the temperature to the room temperature; performing filtering separation to obtain the hydrogenation catalyst, layering reaction liquid to obtain a solvent layer and a glycerin layer, wherein the solvent layer contains a solvent, pentachloroethane, pentachloroethane and trichloroethane, and the glycerin layer contains the glycerin, dichloropropanol, water, the chlorination catalyst and monochlorohydrin.
Chlorohydrination of allyl chloride with HCl and H2O2 catalyzed by hollow titanium silicate zeolite to produce dichloropropanol
Peng, Xinxin,Xia, Changjiu,Lin, Min,Yuan, Hui,Zhu, Bin,Zhang, Yao,Wang, Baorong,Shu, Xingtian
supporting information, p. 1221 - 1225 (2017/08/15)
Overall, over 95% of epichlorohydrin is industrially manufactured via the chlorohydrination route with hazardous Cl2 as a reagent, which brings serious operation and pollution problems. Herein, we describe a novel Cl2-free process for the synthesis of dichloropropanols from allyl chloride with H2O2 and HCl catalyzed by hollow titanium silicate zeolite under mild conditions. A high conversion and overall dichloropropanol selectivity exceeding 95% are simultaneously achieved, and the heterogeneous catalyst is highly stable and amenable for reuse. Comprehensive experimental and spectroscopic data suggest that the Lewis acidity of the framework Ti species has a synergistic effect with the Br?nsted acidity of HCl that promotes the epoxidation of allyl chloride and the ring opening of the epoxy groups.
Method for synthesizing chloropropylene oxide from glycerin
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Paragraph 0017, (2017/01/17)
The invention discloses a method for synthesizing chloropropylene oxide from glycerin. The method comprises a glycerin chlorination reaction and a dichloropropanol saponification reaction. The method comprises the following steps: carrying out a reaction on glycerin at 105DEG C with adipic acid as a catalyst according to a molar ratio of the catalyst to glycerin of 1:23 to obtain highest-yield dichloropropanol, putting a flask with three necks in an oil bath pot, adding dichloropropanol and sodium hydroxide to the flask according to a molar ratio of sodium hydroxide to dichloropropanol of 1:1-1.4:1, carrying out a cyclization reaction at 40-65DEG C for 20-40min, neutralizing the above obtained reaction product with hydrochloric acid, carrying out water vapor distillation, condensing the obtained mixed steam in order to layer the mixed steam, drying the obtained lower layer liquid with anhydrous sodium chloride overnight, carrying out reduced pressure distillation, and collecting a 83-85DEG C/34000Pa fraction. The method for synthesizing chloropropylene oxide, provided by the invention, has the advantages of short time, high income, few steps, simple requirements of the catalyst, low production cost, energy recycling, reduction of the energy consumption and the material consumption, and improvement of the quality of the product.
Method for producing dichlorohydrin through glycerol chlorination
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Paragraph 0025-0027; 0031-0033; 0037-0039; 0043-0045, (2017/04/22)
The invention belongs to the technical field of compound preparation, and particularly relates to a method for producing dichlorohydrin through glycerol chlorination. The method comprises the steps that a catalytic chlorination reaction is conducted by taking glycerol as a raw material and taking HCl as gas through an existing conventional technology, and an active catalyst is prepared by taking compounds of cobalt, compounds of manganese and compounds of iron as active components, taking compounds of zinc as active auxiliaries and applying the active components and the active auxiliaries to the surface of a catalyst carrier. According to the method, positive catalysis of a dichlorohydrin reaction can be effectively catalyzed, and obtained dichlorohydrin (including 1,3-dichlorohydrin and 1,2-dichlorohydrin) is good in selectivity and high in target product yield.
PROCESS FOR HYDROGENATING DICHLOROISOPROPYL ETHER
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Page/Page column 6, (2016/04/20)
Convert dichloroisopropyl ether into a halogenated derivative by contacting the dichloroisopropyl ether with a source of hydrogen and a select heterogeneous hydrogenation catalyst under process conditions selected from a combination of a temperature within a range of from 50 degrees centigrade (oC) to 350 oC, a pressure within a range of from atmospheric pressure (0.1 megapascals) to 1000 pounds per square inch (6.9 MPa), a liquid feed volume flow to catalyst mass ratio between 0.5 and 10 L/Kg*h and a volume hydrogen / volume liquid ratio between 100 and 5000 ml gas/ ml liquid. The halogenated derivative is at least one of 1-chloro-2-propanol and 1,2-dichloropropane 1, and glycerin monochlorohydrin.
A kind of glycerin method of preparing dichlorohydrine chloride
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Paragraph 0021-0023, (2017/05/12)
The invention relates to a method of preparing dichloropropanol by glycerol chlorination, belonging to the field of application of biomas glycerol. The method comprises the following step of: by using a hydrogen chloride gas as a chlorinating agent, by using malic acid, citric acid and lactic acid as a catalyst to catalyze glycerol chlorination to prepare the dichloropropanol. The material glycerol adopted by the method disclosed by the invention is cheap in price, and chloridized to have important industrial significance in developing downstream products. Hydroxyl carboxylic acid is easy to obtain and does not need further treatment; while being used as the catalyst for chlorination, the hydroxyl carboxylic acid has no pollution to environment, is high in catalytic activity, simple in process, gentle in reaction condition, less in dosage of the catalyst and less in reaction byproducts.
Production method for epichlorohydrin
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Paragraph 0070-0071, (2017/03/18)
The invention relates to a production method for epichlorohydrin. The method mainly solves the problems of large amounts of waste water and waste residues, serious pollution and strong corrosiveness to equipment in the prior art. A technical scheme of the invention adopts the production method which comprises the following steps: with chloropropene and ethylbenzene hydroperoxide as raw materials and ethylbenzene as a solvent, subjecting the raw materials and a titanium-contained porous silicon dioxide catalyst to contact reaction so as to obtain epichlorohydrin and alpha-methylbenzyl alcohol under the conditions that reaction temperature is 25 to 200 DEG C; reaction absolute pressure is 0.1 to 8.0 MPa; a molar ratio of chloropropene to ethylbenzene hydroperoxide is 1 to 15; and weight-space velocity of ethylbenzene hydroperoxide is 0.01 to 20 h. Thus, the problem is well solved, and the method can be applied in industrial production of epichlorohydrin.
